Hot melt gasketing compositions and processes for applying them

ABSTRACT

Compositions from 25% to 65% of a synthetic rubber block copolymer and from 75% to 35% plasticizer by weight are heated and mixed and applied, usually with a curing agent, to the lid or cover of a container such as a drum or pail. The application may take place while the lid or cover is revolved and the heated mixture is flowed on. The synthetic rubbers may be of the groups comprising SBS rubber, SIS rubber, S-EB-S rubber. The plasticizer may be from the group comprising paraffin, oils or waxes, polyethylene, polypropylene or ethyl vinyl alcohol. 
     Apparatus is also shown and described for implementing the application of the compositions to the lid or cover as it is revolved. If a groove is formed in the cover before reception of the composition, the apparatus extrudes or flows it into the groove and then the flowed-in material is permitted to set.

This is a continuation-in-part application of the present inventor'sprevious application Ser. No. 440,110, filed Oct. 8, 1982, nowabandoned, and entitled "Hot Melt Gasketing Compound for Drums andPails".

BACKGROUND OF THE INVENTION

A. Field of the Invention

The present invention relates generally to the field of gasketingproducts, compositions and methods, especially to the field of hot-melt,formed-in-place compositions flowed onto containers such as drums andpails made of metal, fiber or plastic.

B. Prior Art

Currently, to provide suitable sealed closures for drums and pails orthe like, it is the usual practice to employ conventional plastisol orrubber latex materials. The latter materials require considerable energy(heat) first to remove water from the compositions while they are beingprepared and then again when the compositions are cured to form thegasket. Gaskets have also been formed by applying liquid plastisolcompositions directly onto lids or closures at room temperature. Thelids are then put into an oven at a temperature of about 420° F. forabout four minutes. Then, to effect post-cure, they are again subjectedto high temperature conditions for a considerable length of time whichentails very large energy usage. Both of the last two steps result inheating the lids to hard-to-handle temperatures.

Conventionally, it is also known to provide or insert apreviously-formed gasket as a separate item between the open end of thecontainer and its lid or cover. In some instances, the previously-formedgasket is secured to the lid or cover by the use of a suitable adhesivematerial that is compatible with the gasket material and with thecontents stored in the container.

Conventional gaskets often do not have the desirable qualities of thegasket products of the present invention. One quality that is oftenlacking is high resistance to compression set. This means that thecontainers presumably closed by such conventional gaskets may in fact behighly susceptible to leaks through the gasket under certain conditions.

Typical gasketing materials that have been employed in the past withvarying degrees of success include soft metal such as copper, andnumerous resilient non-metallic products including cork, rubber,neoprene and other plastic materials. Such materials have includedfluorocarbon polymers, plasticized vinyls, silicone and thermoplasticelastomers.

It is therefore among the objects of the present invention to provide asuperior gasket product which:

1. Has excellent slip and flexibility characteristics.

2. Is resistant to exudation of its constituent components such asplasticizing oils or the like.

3. Has high resistance to compression set.

4. Is made of relatively low cost materials.

5. May be made in a relatively low cost process.

6. Is sparing of heat usage during its fabrication.

7. Can be made in a hot-melt application directly onto the container lidin a short time.

8. Does not require any adhesives to keep it in place relative to theclosure of the container, yet is relatively easy to remove therefrom.

9. Has high resistance to water-soluble materials.

It is also among the objects of the invention to provide:

10. A process for forming gaskets by flowing a fluid having goodviscoelastic properties onto the closure of the drum, pail or othercontainer.

11. A process for forming a gasket in which curing of the gasketcomposition is effected substantially simultaneously with theapplication of the composition to the closure of the container.

12. A process which minimizes the need for long periods of post-curingat quite high temperatures.

SUMMARY OF THE INVENTION

Gasketing compositions comprising 25%-65% of synthetic rubber blockcopolymer and 75%-35% plasticizer are heated, mixed and applied,simultaneously with a curing agent to the lid or cover of a containersuch as a drum or pail while the latter is revolved. Correspondingapparatus is also described.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 is a perspective view of apparatus for forming the gasket inaccordance with the present invention; and

FIG. 2 is a side elevation, partly sectional of part of the apparatusshown in FIG. 1.

DESCRIPTION OF THE INVENTION

The present invention relates to a process for forming, in place, agasket for the lids of drums or pails or the like, and products madefrom the process, as well as compositions of matter used in carrying outthat process to produce a gasket product. In general, the compositionsinvolve a synthetic rubber block copolymer and a plasticizer which aremixed together and flowed-on or otherwise applied to the lid or cover ata predetermined rate. In one embodiment of the invention, especiallywhere the gasket product, in use, is to be subjected to more elevatedtemperatures, a vulcanizing or curing agent may be added to the gasketcomposition while or just before it is flowed onto the cover or lid.

The gasket compositions can be applied both to metal or fiber types andfor pails which have plastic, metal or fiber covers.

It is important in formulating the mixtures which become the gasketcompositions that the proper range of the synthetic rubber constituentbe adhered to. Otherwise, if the percentage of the synthetic rubbercopolymer is too great, the composition will become too viscous to flowat formable temperatures to form the gasket and to permit the ends ofthe flowed-on gasket material to merge into a homogeneous body. If thepercentage of the synthetic rubber is too low relative to the percentageof the plasticizer, the plasticizer may exude from the gasket into thecontainer and thereby may become unfit for the intended use.

For this invention, snythetic rubbers have been chosen in preference tonatural rubber because the latter does not produce a satisfactorycomposition. Natural rubber is incapable of being plasticized to flow atlow enough temperatures to permit obtaining a composition which hasadequate flow characteristics for in-place application and to giveadequate gasketing properties. Many sythetic rubbers are also similarlyexcluded.

In the preferred embodiment, compositions from 25% to 65% of a syntheticrubber block copolymer and from 75% to 35% plasticizer by weight areused to form, in place, a gasket on the lid or cover of a container suchas a drum or pail. These ingredients are mixed under elevatedtemperatures until a homogeneous mass is obtained. The hot melt mixtureis then applied to the lid or cover together with a curing agent whicheffects vulcanization of the mixture in place on the lid. In certaininstances, as will be seen later, the curing agent may not be needed toproduce an acceptable gasket.

The synthetic rubber(s) may be of the group comprising:styrene-butadiene-styrene (SBS rubber), styrene-isoprene-styrene (SISrubber), or styrene-ethylene-butylene-styrene (S-EB-S rubber). Dependingupon the desired viscosity of the composition, varying amounts of theruber constituent(s), up to about 50% thereof by weight, may be replacedwith butyl rubbers, ethylene-propylene rubbers, EPDM rubbers,styrene-ethylene or styrene-butylene rubbers.

In order to facilitage mixing, or adjust viscosity or other flowcharacteristics during formulation or to produce in the formed gasketcertain desired properties such as the proper degree of hardness ortackiness, the plasticizer(s) is mixed with the synthetic rubbercomponent(s) selected from a group comprising paraffin oils or waxes,polyethylene, polypropylene and ethyl vinyl alcohol. The paraffin oilsare desirably less than 1% aromatic, have a viscosity greater than about400 SUS and have a flash point greater than about 400° F.

If the gasket product is not, in use, to be subjected to temperatures inexcess of about 150°-210° F., curing or vulcanization of the flowed-onmixture may not be needed. Where the end use will subject the gasket totemperatures above that range, however, curing may be effected byapplying to the hot-melt mixture just before flowing it on in place, acuring agent selected from the group comprising a peroxide or an azocatalyst. The group may include, for example, benzoyl peroxide, dicumylperoxide, ditertiary butyl peroxide, or azobisisobutyrl nitrile.

The compositions taught in the present invention are thermo-plasticduring their application to the lid or closure and exhibit excellentconsistency and flow. The final gasket product is also quite resistantto compression set and to exudation of any of its components, such asthe plasticizer. The final gasket is also resistant to chemical changeor extraction of any of its components by the contents of the container.With standard conventional gaskets, compression set is undesirably highat temperatures above 210° F. and the prior art required additionalsteps in processing to enhance the gasket's resiliency or flexibility.The present invention does not require these additional processing stepsto achieve higher resistance of the gasket to compression set. Thepresent invention also dispenses with the necessity for using cure ofthe gasket material by electron beam. This conventional type of curingis relatively expensive involving the use of expensive equipment andmore labor. For gaskets for drums it is even possible that the gasketmay be degraded by its use after using the hot-melt plus curing agentprocess described above.

Optionally, a blowing agent, filler, pigment or anti-sticking agent maybe employed in formulating the composition. A suitable foaming orblowing agent such as nitrogen or carbon monoxide gas, ornitrogen-producing agents will produce a formed gasket. The use of azoas a curing and blowing agent and proper use of fillers will assist inproducing a gasket product which has superior resistance to compressionset than those gaskets known to the prior art. The present inventionproduces a gasket product that is resistant to compression set,exudation of the plasticizers and extraction by pail contents.

The following are examples of the formulas and processes used inpreparing the hot melt for application to the lid or cover to make theplastic gasket product.

EXAMPLE 1

37 parts of Solprene 416 (Phillips) synthetic SBS rubber was mixed at270° F. with 57 parts by weight of Sunpar 110 plasticizer (Sun) in anyappropriate chemical mixer together with 6 parts of calcium carbonate asa filler. This heated mixture was applied together with 0.6 parts of aformulation of 50% benzoyl peroxide with a 50% calcium phosphate carrier(also at 270° F.) which helps to prevent flashing of the peroxideitself. To facilitate actual application of the peroxide, some of theparts of the Sunpar 110 are pre-mixed with it prior to applying thecuring agent to the rubber and plasticizer components. This is donewhenever benzoyl peroxide is used in the following examples.

EXAMPLE 2

20 parts Solprene 416, 15 parts Solprene 411, (SBS rubbers) 56 partsSunpar 110 and 9 parts calcium carbonate filler were mixed together asin Example 1 and at the same temperature and in the same type of mixeralthough other mixers can be used as well. Then 0.6 parts of the samecuring agent, benzoyl peroxide on a non-flashing carrier, were added atthe same temperature as before.

EXAMPLE 3

20 parts of Solprene 416, 20 parts Kraton G1650 (a Shell SIS copolymer),55 parts of Sunpar 110 and 5 parts of calcium carbonate were mixedtogether as before at the same temperatures and in the same type ofequipment. 0.6 parts by weight of the benzoyl peroxide was added at thesame temperature just prior to applying the mixture to the lid or cover,or a groove formed therein. Shell's Shel-flex 371 could be substitutedfor Sunpar 110 in about the same concentrations, i.e., 40-68 parts.

EXAMPLE 4

32 parts by weight of Kraton G1650 block copolymer (Shell) were mixedunder the same temperatures with 68 parts of Britol 55P (BrowlerPetrochemical), a plasticizer, and 18 parts of calcium carbonate as wellas 0.6 parts of the benzoyl peroxide curing agent were also applied at270° F.

EXAMPLE 5

36 parts of Kraton G1650 were mixed with 52 parts of Sunpar, 12 parts ofcalcium carbonate and 0.6 parts of the same benzoyl peroxide curingagent, all at the same temperature as in the previous Examples.

EXAMPLE 6

28 parts of Kraton were mixed under the same elevated temperatures with40 parts of Sunpar, 18 parts of Elvax 150 (Dupont), an ethyl vinylalcohol, (a plasticizer), 14 parts of paraffin wax and 0.6 parts of thebenzoyl peroxide curing agent. In formulating the composition, 5% ofdibutyl phthalate may be used to increase the solubiliy of the Elvax.About 10% of polypropylene or polyethylene could be substituted for theparaffin wax for greater hardness of the gasket.

EXAMPLE 7

32 parts of Kraton, 68 parts of Sunpar and 0.6 parts of the same curingagent are processed in the same way as all of the above examples.

EXAMPLE 8

40 parts of Solprene 416, 60 parts of Sunpar 110 were mixed togetherunder the same high temperatures. Then after mixing those completely, 2parts of benzoyl peroxide were added at 270° F. and this cross-linkedall of the other constituents. A variation would be to use, instead ofthe benzoyl peroxide, VUL-CUP curing agent (Hercules) in the same amount(2 parts).

EXAMPLE 9

40 parts Solprene 416, 60 parts Sunpar 110, 2 parts Hysil 233 silica asa filler were mixed in the usual fashion and then, at 270° F. benzoylperoxide (2 parts), or at 300° F. 2 parts of VUL-CUP, were added whichcross-linked the mixed-together components. The Hysil is an oil-acceptorwhich helps to prevent exudation of the plasticizer from the gasket.

EXAMPLE 10

The same ingredients and processing as in Example 9 except for thesubstitution of 10 parts of Solprene 411 for the Hysil 233. The Solpreneimparts greater strength and resistance to compression set of the gasketproduct.

EXAMPLE 11

The same ingredients as in Example 9 except that 6 parts of Hysil 233were used instead of 2 parts of Hysil. They were subjected to the sametemperature and mixing as in Example 9.

Formulations such as those disclosed in Examples 1 through 7 haveresulted in varying degrees of recovery from compression set as measuredby ASTM 395, Method B, which involves heating at 100° F. for threehours. Examples 1-7 had recovery from compression set readings of 62%,58%, 56%, 71%, 40%, 50% and 30%, respectively.

Examples 1, 2 and 3 had Shore A hardness numbers of 18, 21, and 16respectively. Examples 5 and 6 had hardness numbers of 11 and 40respectively.

Elongation characteristics for the first 6 Examples were 300%, 250%,200%, 250%, 300%, and 150%, respectively.

Staining characteristics of kraft paper at -10° C. for Examples 1-6were, respectively, slight, minimal, slight, non-staining, non-staining,and non-staining.

If desired, other components may be added to the hot-melt mix. Forexample, viscosity-reducing agents such as the monomer Saret 500(Sartomer Resins), a trimethacrylate product, may be added in smallquantities such as 0.6 to 1.2 parts. In addition, this monomer increasesthe hardness of the finishsed gasket product.

Other fillers or pigments may likewise be used as desired. Also, toimprove the adhesion of the gasket to the lid, resins of the polyterpeneclass may be added to the hot-melt mix.

As required to produce a foamed gasket, blowing agents such as nitrogenor carbon dioxide may be resorted to.

Also, if desired, foaming or blowing agents such as Celogen OT may beemployed in typical quantities of, say, 2.8 parts.

Apparatus and method suitable for forming a gasket product in accordancewith present invention will now be explained. As shown in FIG. 1, atable 10 is shown on which there is affixed a mechanically rotatableturntable 11 on which a lid 12 is positioned. The turntable is rotatedby an appropriate driving motor (not shown in the drawing) and may bemoved vertically as well. A dispensing head 13 is disposed above theturntable close to its periphery. The nozzle portion 14 of the head 13is positioned over a groove 15 formed in the lid 12. The head isconnected by pipes or tubes 16, 17 and 18 to a pump (not shown) adaptedas described below to supply the hot-melt gasket compositions to it.

A centering subassembly 20, which can be raised or lowered, may bemounted atop the table 10 for rotation in a generally horizontal planein a manner similar to the mounting of the tone arm of a record player.

At the beginning of the gasketing operation, the turntable 11 is in alow position. The cover or lid 12 is placed on the turntable so thattheir centers coincide. Then the turntable is raised towards the nozzle14 so that the groove 12a is below the nozzle.

The centering subassembly has a generally vertical member 21 which canbe aligned with the center of rotation of the turntable. It has an arm22 which has at its lower extremity a disc 23. The disc is mounted toarm 22 by a ball-bearing assembly so that the arm can exert downwardpressure, via the disc, on the lid while the latter is being rotated bythe turntable. The centering subassembly keeps the cover 12 firmly heldduring the gasket-forming stage so that it does not go off-center.

After the cover 12, which may be made of metal, plastic or fiber, isplaced on the turntable, the turntable is raised, the centering arm ispivoted over the turntable and its disc is lowered into contact with theraised cover. The nozzle 14 and the motor for the turntable areconnected to an appropriate timing circuit (not shown) which istriggered by a push button 26 or a foot pedal (not shown). When thebutton is pressed, the timing circuit turns on the motor and the nozzleonly for the time required for the turntable to complete a singlerevolution which can be in as little as, for example, 2 seconds. Bypressing the pushbutton, the turntable and nozzle are activated, and theturntable rotates for one complete revolution while the hot-melt gasketmaterial is deposited into the groove. When the turntable stops, thecentering arm is pivoted back out of the way of the lid or cover; theturntable is lowered. The lid is then removed and put aside while thegasket material sets at room temperature. The process may then berepeated on the next cover.

In the apparatus shown in FIG. 1, the dispensing head 13 including thenozzle 14 may be obtained from Pyles Industries. The head 13 includes,internally, an air-operated valve (not shown) which is open or shut bymeans of air pressure supplied through the two small tubes 16 and 17.This valve allows the hot-melt combination to flow through and out thenozzle 14.

The larger tube 18 has within it near its point of attachment to thehead 13 a static mixing apparatus shown schematically at 19. Upstream ofthe mixer 19 another tube 24 is joined to and in communication with thetube 18. The tube 18 brings the hot-melt liquid from a convenationalhot-melt application equipment, designed for adhesives or the like, suchas the 55 gallon bulk-drum unloader distributed by Kent-Moore PylesIndustries, Inc. or by the Nordson Corporation. This apparatus has aheated subassembly which is dipped into a drum of the previously-mixedblock copolymer-plasticizer as discussed above in connection with thevarious examples.

Through the tube 24, the catalyst or curing agent, as described above inconnection with the various examples, and/or the blowing agent aresupplied at the same approximate temperature as the hot-meltcompositions.

At the dispensing head, the pressure of the combined liquid compositionsis in the 40-80 pounds range with 60 pounds being the average. Thiscontrasts sharply with plastic extruders wherein 1000 pounds per squareinch is a common extruding pressure.

In one satisfactory set of operating conditions, the groove formed inthe cover or lid had a circumference of approximately 671/2 inches, andthe nozzle applied somewhat more than 50 grams of gasket material foreach revolution of the lid at a flow rate of about 350 pounds per hour.The groove itself had an approximate cross-section of 13/4 squareinches.

After the gasket material is flowed into the groove, the lid is setaside to cool at room temperature for several minutes.

In some instances, to improve the resistance to compression set evenmore, the gasket so formed may be heated for two or three minutes at atemperature of about 325° F. This additional heating adds additionalcross-linking to the deposited gasket material.

Gasket products of the type described herein are usually not permanentlyfused to the cover or to the groove in the cover. If the formed gasketproduct is unsatisfactory, it may be removed from the groove simply bypeeling or stripping it therefrom with relatively little effort. A newgasket may then be formed on the cover or in the groove of the cover asexplained above.

What is claimed is:
 1. A method of forming a gasket on the lid or coverof a container such as a drum or pail or the like, comprising:(a)providing a hot-melt composition which comprises 25%-65% by weight ofsnythetic rubber copolymers mixed with 75%-35% of a plasticizer, (b)rotating said cover or lid, (c) applying said composition to said coveror lid while rotating, said rotation being at a speed low enough toprevent centrifugal force from causing dispersion of the appliedcomposition, and (d) permitting said applied composition to set.
 2. Themethod according to claim 1 wherein a curing composition is brought intocontact with the first-named composition just prior to applying saidfirst composition to said cover or lid.
 3. The method according to claim2 wherein said curing composition is selected from the group comprisinga peroxide or an azo catalyst.
 4. The method according to claim 3wherein said peroxide is selected from the group comprising benzoylperoxide, dicumyl peroxide, or ditertiary butyl peroxide.
 5. The methodaccording to claim 1 wherein there is a gasket-forming groove formed insaid lid and wherein said composition is applied to said groove at about40-80 pounds per square inch and at a temperature in the range of about275°-325° F.
 6. The process of forming, in place, a gasket for acontainer having a lid or the like, which comprises:(a) providing a hotfluid composition which comprises 25%-65% by weight of synthetic rubbercopolymers mixed with 75%-35% of a plasticizer, (b) providing a curingcomposition for said (a) composition, (c) bringing said (a) and (b)compositions together, and (d) immediately applying saidbrought-together compositions to a predetermined portion of said lid orthe like.
 7. The process according to claim 1 with the addition of step(e) permitting said applied compositions to cool.
 8. The processaccording to claim 6 wherein the application of said brought-togethercompositions is by flowing said last-named compositions onto saidpredetermined portion of the container.
 9. The process according toclaim 8 wherein said predetermined portion comprises a groove in saidlid or the like.
 10. The process according to claim 8 wherein said lidor the like is turned while said application of said brought-togethercompositions thereto is effected.
 11. The process according to claim 8wherein said application of said brought-together compositions is madewhile they are at a temperature in excess of about 275° F.
 12. Theprocess according to claim 6 wherein said synthetic rubber copolymer isselected from the group comprising styrene-butadiene-styrene rubber,styrene-isoprene-styrene rubber, or styrene-ethylene-butylene-styrenerubber.
 13. The process according to claim 6 wherein up to about 50% byweight of said rubber content is replaced by rubber selected from thegroup comprising butyl rubbers, ethylene-propylene rubbers, EPDMrubbers, styrene-ethylene or styrene-butylene rubbers.
 14. The processaccording to claim 6 wherein said plasticizer is selected from the groupcomprising paraffin oils or waxes, polyethylene, polypropylene and ethylvinyl alcohol.
 15. The process according to claim 14 wherein saidparaffin oils or waxes have a SUS viscosity greater than about
 400. 16.The process according to claim 14 wherein said paraffin oils or waxeshave a flashpoint greater than about 400° F.
 17. The process accordingto claim 14 wherein said paraffin oils or waxes are less than 1%aromatic.
 18. The process according to claim 6 wherein said curing agentis selected from the group comprising a peroxide or an azo catalyst. 19.The process according to claim 18 wherein said peroxide is selected fromthe group comprising benzoyl peroxide, dicumyl peroxide, or ditertiarybutyl peroxide.
 20. The process according to claim 18 wherein said azocatalyst comprises azobisisobutyrl nitrile.
 21. A method according toclaim 1 wherein said applied composition is permitted to set at ambienttemperature.
 22. A method according to claim 7 wherein said appliedcomposition is permitted to cool at ambient temperature whereupon agasket is formed on said lid or the like.
 23. A method according toclaim 1 wherein the said step (c) is initiated while said cover or lidis at ambient temperature.
 24. A method according to claim 23 whereinsaid step (c) is performed at ambient pressure.
 25. A method accordingto claim 23 wherein said step (d) is performed at ambient pressure andno pressure is thereafter applied.
 26. A method according to claim 21wherein said composition is non-volatile.
 27. A method according toclaim 6 wherein said composition is non-volatile.
 28. A method offorming a gasket on the lid or cover of a container such as a drum orpail or the like, comprising:(a) providng a hot-melt composition whichcomprises 25%-65% by weight of synthetic rubber copolymers mixed with75%-35% of a plasticizer, (b) applying said composition while impartingrelative rotation between said lid or cover and the point where saidapplying occurs, said applying being at a speed such as not to causesubstantial dispersion of said composition on said cover or lidsubsequent to its coming into contact therewith, and (c) permitting saidapplied composition to set.
 29. A method according to claim 1 whereinsaid composition sets by having its temperature lowered.
 30. A methodaccording to claim 1 wherein said copolymers are synthetic rubber blockcopolymers.
 31. A method according to claim 6 wherein said copolymersare synthetic rubber block copolymers.
 32. A method according to claim 1wherein said gasket does not exude said plasticizer.